Engineering of Calcium Alginate- PANI@Sawdust Wood hydrogel Bio-beads for the Removal of the Sulfonate Groups-Containing Orange G dye from Aqueous Solution

doi:10.21203/rs.3.rs-979902/v1

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Engineering of Calcium Alginate- [email protected] Wood hydrogel Bio-beads for the Removal of the Sulfonate Groups-Containing Orange G dye from Aqueous Solution

https://doi.org/10.21203/rs.3.rs-979902/v1

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The aim of this work is to investigate the adsorption performance of orange G (OG) dye from aqueous solutions employing [email protected] biocomposite enrobed by calcium-alginate biobeads ([email protected]). The as-prepared adsorbent was characterized by scanning-electron-microscopy (SEM), X-ray energy dispersive spectroscopy (EDS) and Fourier transforms infrared (FT-IR) spectroscopy, and used to remove Orange G dye from water. batch tests were performed as a function of adsorbent dosage, pH, contact time, interfering ions and initial OG dye concentration. Experimental results show that the kinetic model of pseudo-first-order (PFO) and Freundlich isotherm provided a good fitting of the whole experimental data. The results revealed that the as-prepared tricomposite [email protected], has the potential to be applied as a low-cost adsorbent for the adsorption of OG dye from aqueous media.

Environmental Chemistry

Toxicology

Calcium alginate

[email protected]

sawdust wood

biobeads

OG dye removal

The rapid influx of people growing creates a clean-water challenge, that is already being confronted in the world (Chang et al. 2016; Pradhan et al. 2020). The water pollution threat could be caused by industry such as the release of dyes into the environment in the form of wastewater (Salam et al. 2017; Yeamin et al. 2021). The occurrence of dyes, even at low concentrations, in water adversely affects human health and is toxic to the life of microorganisms and their biological systems (Zheng et al. 2019). Various dyes resist biodegradation due to their aromatic structure. Among the dyes, Orange G (OG) is generally used in textile tanneries. OG dye is one of the azo dyes and could be cause irritation to the skin, eyes and mucous membranes, respiratory organs and cancer (Imgharn et al. 2021). Therefore, the elimination of dyes from contaminated water is necessary before their release into the natural environment. For this purpose, several techniques have been developed, such as chemical precipitation (Singh and Chauhan 2009), photodegradation processes (Miklos et al. 2018; Naciri et al. 2021), coagulation-flocculation (El-Gaayda et al. 2021), ion exchange and adsorption processes (Grzegorzek et al. 2020; Laabd et al. 2021; Hsini et al. 2021b). The superiority of adsorption separating pollutants owing to the flexibility in design and system, and good output performance in several cases, the capability to reuse the adsorbent in several times, and the low cost of process (Hsini et al. 2021a; Laabd et al. 2021) .

A large collection of biosorbents or biomaterials from natural sources like almond shells, walnut shells, bagasse sugarcane, sawdust, and biomass made up of living, or dead microorganisms, and biopolymers were employed as adsorbents to adsorb contaminants from aqueous solutions, owing of their low cost, availability and their adsorption capacity to treat wastewater (Hsini et al. 2020). However, all these materials provide a simple uptake of contaminants. In order to anhance the adsorption performance of biomaterials, conducting polymers have been increasingly used for their adsorption capability and the polyaniline (PANI) is the most efficient among them (Laabd et al. 2022). Because of its porous structure, regenerability and ion exchange capacity, as well as a large number of amine/imine groups.

Polysaccharide alginate is commonly obtained from brown seaweed. As a biopolymer, sodium alginate is largely applied in pharmaceuticals, cosmetic and hygienic products, textiles, food additives and dyes (Rocher et al. 2008). This polymer has very long-chain molecules with active carboxylic groups that can be straightened along with each other in a way to be in line with the capability to create a leaf material. One of the tunable qualities of alginate is the capacity to build a hydrogel (Dąbrowski et al. 2005; Javanbakht and Shafiei 2020). An aqueous alginate solution is easily crystallized into a hydrogel, plus double metal cations such as Ca²⁺.

The main purpose of the current work is to the encapsulation of [email protected] biocomposite in calcium alginate biobeads as a new eco-friendly adsorbent for OG dye adsorption from aqueous media. The engineered biobeads were characterized by SEM, EDX and FT-IR analyses. Batch testts were carried out for Orange G molecules removal experiments using the prepared biobeads. The effect of contact time, adsorbent doses, pH, initial OG dye concentration, and the co-interfernig ions, kinetics, isotherm studies were evaluated.

2.1. Engineering of [email protected] biobeads

The Sawdust was washed and then air-dried for 4 days. The dried sawdust was crushed and sieved. This SD powder was washed with distilled water and then dried in an oven at 80°C for 24h.

PANI composite was synthesized applying in situ polymerization of aniline monomer in the occurrence of SD particles (Imgharn et al. 2021). In a typical procedure, 1g of SD powder and 1 mL of distilled aniline monomer were added to 80 mL of HCl (1 M). The mix was sonicated for 1 h and the kept under stirring for 3 h. Afterward, sodium persulfate was dissolved in 40 mL of the HCl (1 M) solution and added drop-wise to the suspension under stirring for 6 h at 298K. The resultant precipitate was leached with deionized water and acetone. Finally, the precipitate ([email protected]) was dried at 80°C overnight.

For the fabrication of the [email protected] biobeads, the 1:1 weight ratio of the synthesized [email protected] biocomposite and sodium alginate was added to 50 ml distilled water and kept under stirring for 3 h until the formation of a viscose gel. In order to form the biobeads, we added dropwise using a syringe with a 4 cm distance between the needle and the solution surface, the gel to the solution of 0.5 M calcium chloride 0.5 M as cross-linker. The prepared [email protected] biobeads were stirred for 30 min, then the final biobeads were washed with distilled water.

2.2. Characterization of [email protected] biobeads

Morphological analysis was analyzed by scanning electron microscopy (SEM, JEOL, JSM-IT200) coupled energy dispersive spectroscopy (EDS). Fourier-transform infrared (FTIR) spectra of the obtained samples were documented on KBr pellets using FT-IR spectroscopy (ALPHA-Bruker Optics, Germany) wavenumber range from 400 to 4000 cm⁻¹.

The point zero of charge (pH_PZC) was defined by a conventional technique, which involves preparing 60 ml solutions of KNO₃ (0.03 M) and modifying their pH to accurate values (2 – 10). Next, 0.45 g of biobeads were added to every solution. The mix was kept under stirring at ambient temperature for 24 h before calculating the pH_final. The pH_PZC was computed from the curve of pH_final-pH_initial = f(pH_initial).

2.3. Batch experimental studies

In a series of 100 ml beakers, 50 ml of aqueous solutions of OG with specified concentrations were added into a defined amount of biobeads in order to conduct the adsorption measurements. The mix was stirred at 120 rpm and under a constant temperature of 298K for 180 min. At a fixed time, the stirring was stopped, and the samples were centrifuged. The OG dye residual concentration in the reaction mix was evaluated via UV2300 spectrophotometer. Adsorption tests were performed by changing initial solution pH, contact time, adsorbent dose, co-interfering ions and initial OG concentration for adsorption kinetics and adsorption isotherm.

The adsorbed amount of dye onto the adsorbents at time t is Q_t was determined by the following equation (Shuang et al. 2012; Essekri et al. 2021):

$$R\left(\text{%}\right)=\frac{\left({C}{0}-{C}{e}\right)}{{C}_{0}}\times 100 \left(1\right)$$

Furthermore, the dye elimination efficiency, i.e., percent of adsorption, was examined as:

$${Q}{e}=\frac{\left({C}{0}-{C}_{e}\right)}{m}\times V \left(2\right)$$

C₀ is the initial OG dye concentration (mg/L), C_t is the concentration of OG dye at time t, V is the volume of OG dye containing-solution (L), and m is the mass of adsorbents in g. Experiments at the equilibrium were carried out via the above process with a broad array of initial dye concentration. The time of contact between solid-liquid was 180 min, which was higher than the equilibrium time.

3.1. Characterization of [email protected] biobeads

3.1.1. Texture morphology

SEM investigation associated with EDX was figured out the morphologies and chemical composition of SD, [email protected] and [email protected] biobeads as shown in Fig. 1 (a-c). As shown in Fig. 1 (a-c), the SEM images presente that the SD particle has a heterogeneous and porous texture, while the SEM image of the [email protected] biocomposite suggests that the sawdust surface has been successfully enrobed by PANI particles, conducting to the generation of pores within the [email protected] composite structure. These pores may ease the diffusion of sulfonate groups (–SO₃Na)-containing OG molecules into the [email protected] surface. Therefore, SEM image of the [email protected] biobeads depicts that the [email protected] particles were inside a layer formed by alginate and calcium alginate ions allowing the construction of spherical biobeads.

The elemental compositions obtained from the EDX analysis are presented in fig. (d-e). The EDS analysis spectrum of SD (Figure 1 (d)) depicts that the sawdust contains mainly carbon and oxygen elements. Figure III-1 e confirms the occurrence of all the atoms attributing to sawdust (C and O) as well as those of polyaniline polymer like nitrogen (N), and sulfur (S) for [email protected] biocompsite. Moreover, [email protected] biobeads showed the existence of elements corresponding to [email protected] biobeads with the appearance of the other two elements returning to the alginate/Ca²⁺ complex formed.

3.1.2. FT-IR Analysis

The structural characteristics of sawdust (SD), [email protected] and [email protected] biobeads were figured out employing FTIR spectroscopy technique. The spectra of SD, [email protected] and [email protected] are given in Fig. 2, respectively.

In the spectrum of SD, we notice a band at 3427 cm⁻¹ is ascribed to the stretching vibration of O-H groups, the peak centered at 3000 cm⁻¹ are owing to the C-H stretching vibrations and specify the occurrence of alkanes. The band at 1721 cm⁻¹ attibutes to the stretching vibration of C=O groups. The stretching vibration of C=C asigned at 1511 cm⁻¹ is assigned the presence of aromatics. The weak bands 700 cm⁻¹ attribute to the aromatic components along with C-H bending (Liu and Sun 2011; Varma et al. 2019). The FTIR spectrum of [email protected] biocomposite depicts peaks at 1595 cm⁻¹ and 1493 cm⁻¹ ascribing to the typical C=C stretching of quinoid and benzenoid rings, respectively. The occurrence of these two bands indicates the synthesis of PANI and the presence of its amine and imine groups (Joubert et al. 2010). The band at 1306 cm⁻¹ corresponds to the N-H bending mode. The peak at 822 cm⁻¹ could be attributed to the C-H bending in the benzene ring of [email protected] The degree of electron delocalization in the quinoid ring of [email protected] is disclosed by the strong peak around 1145 cm⁻¹. The absorption band asigned at 624 cm⁻¹ is associated with the valence vibration of the C-C bond (Imgharn et al. 2021). These findings provide qualitative information by disclosing the deposition of PANI on the sawdust surface. The FTIR spectrum of biobeads displayed peaks around 1087, 1515, 2925, and 3420 cm⁻¹ which are ascribed to the tensile vibrations of -COH and -COO- (symmetric), C-H bond relates to the functional group of alkenes and O-H stretching, respectively (Javanbakht and Shafiei 2020). These results show that the beads of the alginate /Ca²⁺ layer were coated with the [email protected] particles.

3.2. Adsorption study

3.2.1. Influence of adsorbent dosage and Effect of initial pH

To clear up the adsorption process, it is crucial to investigate the parameters influencing the adsorbate-adsorbent interface. The adsorbent dose effect of [email protected] biobeads on the removal of OG dyestuff was studied and presented in Fig. 3. From the Fig. 3, it is obvious that the OG dye adsorption efficiency depends on the amount of [email protected] biobeads. The percentage of OG dye removal increases as the adsorbent dosage ratio (from 0.5 to 4 g L⁻¹) increases, which is due to the raise in the amount of available binding sites (Liu and Sun 2011; Zheng et al. 2019). The maximum OG dye removal efficiency value of 86.31% was reached for an [email protected] dose of 2.5 g L⁻¹. Above 2.5 g L⁻¹, the number of active sites was competent to approximately remove the OG dye from the medium, thereby reflecting irrelevant changes in OG dye adsorption percentage. This removal trend could be elucidated by the overlapping of active sites generated by the congregating of adsorbent particles under high [email protected] dosage conditions. Thus, 2.5 g L⁻¹ is applied as the optimal adsoebent dose for further adsorption tests.

The pH of solution is a crucial that acts on the adsorption ability by altering the surface capability of the adsorbent and the existing form of adsorbate (Yeamin et al. 2021; Ait Haki et al. 2021). The PZC and the solution pH effect on the adsorption of the OG dye on Alg-PANI @ SD were studied in the pH range from 2 to 10 and illustrated in Fig. 3(b-c), respectively. The PZC point was found to be 5.5, this finding means that the [email protected] biobeads surface charged positively at pH values less than the PZC point (pH<PZC) and vice versa. Mainly, the maximum OG dye removal efficiency (94.7%) was reached at pH=2. As far, the OG dye removal favorability at pH<PZC could be suggested as the result of electrostatic attractions between sulfonate groups (–SO₃Na)-containing-OG molecules and the [email protected] biobeads surface. However, at pH values above the PZC value, the removal of the OG dye gradually decreases as pH increases. This lower affinity for the OG dye may be related to repellency forces. In addition, the pH value 5.0 was selected as an optimal value for further adsorption experiments.

3.2.2. Effect of interfering ions

To figure out the proportional aspects of various competing ions on sulfonate groups (–SO₃Na)-containing OG adsorption on [email protected] biobeads, the influence of co-existing Cl⁻, SO₄²⁻, CO₃²⁻ and NO₃⁻ interfering ions were assessed at initial concentrations (100mg L⁻¹) (Abdellaoui et al. 2021). Fig. 4 depicts the interfering ions effect on the OG dye removal percentage by [email protected] biobeads. It was assigned that the elimination of OG dye was not influenced by the presence of SO₄²⁻, Cl⁻ and NO₃⁻ ions. In contrast, the presence of CO₃²⁻ ions affects the removal efficiency of OG dye. This carbonate competing trend could be attributed to the producing of hydroxide ions by hydrolysis, which in turn contest for SO₃Na-containing OG binding sites or decrease the solution acidity (Vickers 2017).

3.2.3. Adsorption kinetics

The adsorption kinetic of OG dye onto [email protected] biobeads was performed to investigate the relationship between contact time and adsorption capacity for insight into the OG molecule's adsorption process and to provide relevant conditions for the efficient application of [email protected] biobeads adsorbent (Mahi et al. 2021). As can be seen in Fig. 5, the OG dye starts to adsorb rapidly onto [email protected] biobeads within the first contact hour owing to the availability of OG adsorption vacant sites. Thereafter, the OG dye removal rate becomes slower until attaining the equilibrium adsorption after 180 min, as a result of the reduction in the number of sulfonate groups (–SO₃Na)-containing OG dye-binding sites. Pseudo-first-order (PFO) and pseudo second-order (PSO) kinetic models were empolyed to assess the reaction kinetics (Zheng et al. 2012; Amjlef et al. 2021). The nonlinear expressions and the fitting parameters data of PFO and PSO kinetic models are presented in Table 1 and Fig. 5(a). The correlation coefficient (R² ) values indicate that the PFO model (R²=0.996) is more favorable than the PSO one (R²=0.995) for OG dye removal on [email protected] biobeads. Furthermore, the adsorption capacity, calculated from the PFO model (4.468 mg g⁻¹), was found to be close to the experimentally-determined one (4.301 mg g⁻¹), confirming that the OG dye adsorption process was better described by this kinetic model.

Table 1

Parameters of PFO and PSO models for OG removal onto [email protected] from aqueous medium.
Q_e.exp (mg.g⁻¹)	PFO model ${Q}_{t}={\text{Q}}_{\text{e}}(1-\text{e}\text{x}\text{p}(-{k}_{\text{P}\text{S}\text{O}}\text{t}\left)\right)$			PSO model ${Q}_{t}=\frac{{\text{Q}}_{\text{e}}^{2}{\text{k}}_{\text{P}\text{S}\text{O}}t}{1 + {{\text{Q}}_{\text{e}}\text{k}}_{\text{P}\text{S}\text{O}}t}$
	k₁	Q_e.1	R²	k₂	Q_e.2	R²
4.301	0.0157	4.468	0.996	0.0025	5.799	0.995

3.2.4. Adsorption equilibrium

The equilibrium adsorption isotherm is indispensable to figure out the distribution of OG dye molecules at the [email protected] surface, when the adsorption gets to the equilibrium (Feng et al. 2020). Therefore, the analysis by Langmuir and Freundlich isothermal models was carried out (Salam et al. 2017), their nonlinear equations and equilibrium data were displayed in Table 2, and their fitting curves are plotting in Fig. 5(b). According to the correlation values, this figure discloses that the OG dye removal onto the [email protected] biobeads, was well fitted with the Freundlich model (R² =0.991), more than the Langmuir one (R² =0.949). This assumes that the OG dye removal onto the heterogeneous as-synthesized biobeads surface was carried out in multilayer.

Table 2

Nonlinear fitting parameters of Langmuir and Freundlich models for OG adsorption on the [email protected] biobeads.
Q_exp (mg.g⁻¹)	Langmuir ${\mathbf{Q}}_{\mathbf{e}}=\frac{{\mathbf{Q}}_{\mathbf{m}\mathbf{a}\mathbf{x}}{\mathbf{K}}_{\mathbf{L}}{\mathbf{C}}_{\mathbf{e}}}{1+{\mathbf{K}}_{\mathbf{L}}{\mathbf{C}}_{\mathbf{e}}}$			Freundlich ${\mathbf{Q}}_{\mathbf{e}}= {\mathbf{K}}_{\mathbf{F}}{\mathbf{C}}_{\mathbf{e}}^{1/\mathbf{n}}$
Q_exp (mg.g⁻¹)	Q_max (mg.g⁻¹)	K_L (L.mg⁻¹)	R²	n_f	K_F (mg.g⁻¹)	R²
8.03	7.42	0.807	0.949	4.807	3.746	0.991

In this current paper, [email protected] biobeads were prepared and applied as were efficient adsorbent to remove OG dyestuff from the aqueous phase. The adsorbent was characterized for the analysis of the surface properties. It was concluded that OG adsorption was affected by several operating factors like adsorbent dosage, pH, contact time and initial OG dye concentration. The adsorption equilibrium was achieved within 180 min at pH 5.0. The OG dye adsorption process on the [email protected] biobeads was followed by pseudo-first order kinetics. The isotherm modeling revealed an appropriate fitting of the Freundlich isotherm. The electrostatic interactions between sulfonate groups (–SO₃Na)-containing OG dye molecules and [email protected] biobeads surface played a primordial role in the adsorption prcocess. In view of the strong adsorption ability of the adsorbent [email protected] biobeads over OG dye, easy separability, the present study submits that [email protected] biobeads is a novel, effective, and economically feasible for the adsorption of dyes from wastewater containing OG dyestuff.

Ethics approval

This study was approved by the research ethics committee of Ibn zohr university.

Consent to participate

All the authors participed in this article

Consent for publication

All the authors agreed this article be published.

Authors Contributions

Abdelaziz Imgharn: Conceptualization, Methodology, Formal analysis, Investigation, Data curation, Writing-original draft. Nouh Aarab: Participation in the design. Abdelghani Hsini: Writing - review & editing, Investigation, Methodology. Yassine Naciri: Writing - review & editing, Investigation, Methodology. Mahmoud Elhoudi: Investigation, Methodology. Mohamed Ait Haki: Writing - review & editing. Mohamed Laabd: Conceptualization, Validation, Writing - review & editing, Investigation, Methodology. Rajae Lakhmiri: Supervision. Abdallah Albourine: Conceptualization, Supervision.

Funding

This study was not approved and financially supported.

Competing interests

The authors declare no competing interests.

Availability of data and materials

Data and materials are available.

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Engineering of Calcium Alginate- [email protected] Wood hydrogel Bio-beads for the Removal of the Sulfonate Groups-Containing Orange G dye from Aqueous Solution

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1. Introduction

2. Materials And Method